1、Designation: E1363 13Standard Test Method forTemperature Calibration of Thermomechanical Analyzers1This standard is issued under the fixed designation E1363; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision
2、. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method describes the temperature calibrationof thermomechanical analyzers from 50 to 1100C. (SeeNote 1.)1.2 The values st
3、ated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.3 This standard is similar to ISO 113591 but addresses alarger temperature range and utilizes additional calibrationmaterials.1.4 This standard does not purport to address all of thesafety co
4、ncerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. Specific precau-tionary statements are given in Section 7 and Note 10.2. Refere
5、nced Documents2.1 ASTM Standards:2E473 Terminology Relating to Thermal Analysis and Rhe-ology2.2 Other Standards:3ISO 113591 Thermomechanical Analysis (TMA)-Part 1:General Principles3. Terminology3.1 Definitions:3.1.1 The terminology relating to thermal analysis appear-ing in Terminology E473 shall
6、be considered applicable to thisdocument.4. Summary of Test Method4.1 An equation is developed for the linear correlation of theexperimentally observed program temperature and the actualmelting temperature for known melting standards. This isaccomplished through the use of a thermomechanical analyze
7、rwith a penetration probe to obtain the onset temperatures fortwo melting point standards.An alternate, one-point method oftemperature calibration, is also given for use over very narrowtemperature ranges. (See Note 2.)NOTE 1This test method may be used for calibrating thermomechani-cal analyzers at
8、 temperatures outside this range of temperature. However,the accuracy of the calibration will be no better than that of thetemperature standards used.NOTE 2It is possible to develop a more elaborate method oftemperature calibration using multiple (more than two) fusion standardsand quadratic regress
9、ion analysis. Since most modern instruments arecapable of heating rates which are essentially linear in the region of use,the procedure given here is limited to a two-point calibration.5. Significance and Use5.1 Thermomechanical analyzers are employed in theirvarious modes of operation (penetration,
10、 expansion, flexure,etc.) to characterize a wide range of materials. In most cases,the value to be assigned in thermomechanical measurements isthe temperature of the transition (or event) under study.Therefore, the temperature axis (abscissa) of all TMA thermalcurves must be accurately calibrated ei
11、ther by direct reading ofa temperature sensor or by adjusting the programmer tempera-ture to match the actual temperature over the temperature rangeof interest.6. Apparatus6.1 Thermomechanical Analyzer (TMA), The essential in-strumentation required to provide the minimum thermome-chanical analytical
12、 or thermodilatometric capability for thismethod includes:6.1.1 A Rigid Specimen Holder or Platform, of inert, lowexpansivity material ( 1 m m-1K-1) to center the specimen inthe furnace and to fix the specimen to mechanical ground.6.1.2 A Rigid (expansion compression, flexure, tensile, etc.)Probe, o
13、f inert, low expansivity material ( 1 m m-1K-1) thatcontacts with the specimen with an applied compressive ortensile force. For this test method the use of a penetration probeis recommended.1This test method is under the jurisdiction ofASTM Committee E37 on ThermalMeasurements and is the direct resp
14、onsibility of Subcommittee E37.10 onFundamental, Statistical and Mechanical Properties.Current edition approved April 1, 2013. Published May 2013. Originallyapproved in 1990. Last previous edition approved in 2008 as E1363 08. DOI:10.1520/E1363-13.2For referenced ASTM standards, visit the ASTM websi
15、te, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036, http:
16、/www.ansi.org.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States16.1.3 A Sensing Element, linear over a minimum range of 2mm to measure the displacement of the rigid probe to 6 50 nmresulting from changes in the length/height of the spec
17、imen.6.1.4 A Weight or Force Transducer, to generate a constantforce of 50 6 5 mN (5.0 6 0.5 g) that is applied through therigid probe to the specimen.NOTE 3The recommendation of a 5.0 g load (or a force of 50 mN) isbased on the use of penetration probes commonly used in the commer-cially available
18、thermomechanical analyzers. These probes have tipdiameters ranging from 0.89 to 2.0 mm and lead to pressures from 80 to16 kPa when using the recommended 5.0 g load. The use of probes whichdiffer greatly from this range of tip diameters may require differentloading (or force).6.1.5 A Furnace, capable
19、 of providing uniform controlledheating (cooling) at a rate of 1 to 10 6 1C min-1of aspecimen to a constant temperature within the applicabletemperature range of this methodNOTE 4The temperature range of operation of commercial thermo-mechanical analyzers vary by manufacturer and mode. The completer
20、ange of temperature of an instrument is sometimes achieved by the use oftwo different furnaces. In this case, temperature calibration must becarried out for each furnace.6.1.6 A Temperature Controller, capable of executing aspecific temperature program by operating the furnace betweenselected temper
21、ature limits at a rate of temperature change of10 6 1C min-1.6.1.7 A Temperature Sensor, that may be positioned in closeproximity to the test specimen to provide an indication of thespecimen/furnace temperature to within 60.1C min6.1.8 A means of sustaining an environment around thespecimen with an
22、inert purge gas (for example, nitrogen,helium, argon, etc.) at a purge gas flow rate of 20 to 50 mLmin-1.6.1.9 A Data Collection Device, to provide a means ofacquiring, storing, and displaying measured or calculatedsignals, or both. The minimum output signals required forTMAare a change in linear di
23、mension, temperature, and times.7. Hazards7.1 This test method may involve the use of hazardousmaterials, operations, and equipment. It is the responsibility ofthe user of this test method to establish appropriate safetypractice and to determine the applicability of regulatorylimitations prior to us
24、e. (WarningToxic or corrosiveeffluents, or both, may be released when heating some mate-rials and could be harmful to personnel and the apparatus.)7.2 Once this calibration procedure has been executed asdescribed in 10.1.2.1-10.1.2.7 of this test method, the measur-ing temperature sensor position sh
25、ould not be changed, norshould it be in contact with the sample or sample holder in away that would impede movement. If for some reason thetemperature sensor position is changed or the temperaturesensor is replaced, then the entire calibration procedure shouldbe repeated.8. Calibration8.1 For the te
26、mperature range covered by manyapplications, the melting transition of 99.99 % pure materialsmay be used for calibration. (See Table 1.)NOTE 5The melting temperatures of these materials have beenselected as primary fixed points (see Table 1) for the InternationalPractical Temperature Scale of 1990.4
27、NOTE 6Some materials have different crystalline forms (for example,tin) or may react with the container. Such calibration materials should bediscarded after their initial melt.9. Assignment of the Penetration Onset Temperature9.1 The assignment of the TMA penetration onset tempera-ture is an importa
28、nt procedure since, when using this method,temperature calibration of the thermomechanical analyzer isdirectly dependent upon it. The temperature standards given inTable 1 will give a downward deflection on the thermal curve,similar to that shown in Fig. 1, when placed under a weightedTMA penetratio
29、n probe and heated to their respective meltingtemperatures.9.2 The extrapolated onset temperature for such a penetra-tion thermal curve is obtained by extending the pretransitionportion of the thermal curve to the point of intersection with a4Supporting data have been filed at ASTM International Hea
30、dquarters and maybe obtained by requesting Research Report RR:E37-1011.TABLE 1 Recommended Melting Temperature ReferenceMaterialsACalibration MaterialBMelting Temperature(C) (K)Mercury 38.8344 234.3156Water 0.01 273.16Gallium 29.7646 302.9146Indium 156.5985 429.7485Tin 231.928 505.078Zinc 419.527 69
31、2.677Aluminum 660.323 933.473Silver 961.78 1234.93Gold 1064.18 1337.33Copper 1084.62 1357.77AThe values in Table 1 were determined using special, 99.9999 % pure materials,and highly accurate steady state conditions that are not attainable or applicable tothermal analysis techniques. The actual preci
32、sion of this test method is given inSection 12.BB. W. Mangnum and G. T. Furukawa, “Guidelines for Realizing the InternationalTemperature Scale of 1990 (ITS-90),” National Institute of Standards and Tech-nology Technical Note 1265, 1990, p. 8.FIG. 1 Assignment of the Extrapolated Onset Temperature (T
33、o)from TMA Thermal CurveE1363 132line drawn tangent to the steepest portion of the curve whichdescribes the probe displacement. The temperature correspond-ing to this point of intersection is the penetration onsettemperature. This is shown graphically in Fig. 1. There aresome materials (for example,
34、 aluminum metal) which showpretransition probe displacement prior to the sharper down-ward deflection observed on melting. In this case, the pretran-sition baseline is extended from the point which represents thehighest temperature the material reaches prior to exhibitingsignificant or measurable so
35、ftening under the conditions of theexperiment. Fig. 2 describes the assignment of the extrapolatedonset temperature for a specimen which exhibits pretransitionpenetration.10. Procedure10.1 Two-Point CalibrationFor the purposes of thisprocedure, it is assumed that the relationship between observedext
36、rapolated onset temperature (To) and actual specimen tem-perature (Tt) is a linear one governed by the equation:Tt5 To3S!1I (1)where S and I are the slope and intercept of a straight line,respectively.10.1.1 Select two calibration reference materials near thetemperature range of interest. The standa
37、rds should be as closeto the upper and lower temperature limits used in the actualanalysis runs as is practical.10.1.2 Determine the apparent extrapolated onset tempera-ture for the calibration reference material chosen, using apenetration-type probe with the TMA instrument.10.1.2.1 Place a 10 to 20
38、-mg specimen of one of thecalibration reference material on the sample platform (orholder, whichever is applicable).NOTE 7The specimen should have a smooth surface on both top andbottom. Avoid the use of specimens with sharp ridges and irregularsurfaces. These can lead to false values for the onset
39、temperatures.Powdered or liquid standards may be placed into a stable, inert container,if necessary.10.1.2.2 Place a probe loaded with 5 g (or force of 50 mN)in contact with the test specimen.10.1.2.3 Purge the specimen chamber area with inert gas ata flow rate that is appropriate to the dimensions
40、of theapparatus throughout the experiment. Typical flow rates arefrom 20 to 50 mL/min. The same purge gas and flow rateshould be maintained in both calibration runs and analysesruns.10.1.2.4 Heat the calibration sample specimen to a tempera-ture about 50C below the calibration temperature and allowt
41、he TMA furnace to equilibrate.10.1.2.5 Heat the calibration specimen at 5C/min throughthe transition allowing the probe to reach a point of maximumpenetration. (See Fig. 1.)NOTE 8Temperature calibration may be affected by heating rate,purge gas flow rate, and choice of purge gas.NOTE 9Other heating
42、rates may be used but shall be reported.10.1.2.6 From the TMA thermal curve obtained, assign theextrapolated onset temperature (see Fig. 1) to the requiredprecision.NOTE 10Retain all available digits.10.1.2.7 Repeat the procedure described in 10.1.2-10.1.2.5using the second calibration reference mat
43、erial that was cho-sen.11. Calculation11.1 Using the reference material temperature values fromTable 1 and the corresponding onset temperatures obtainedexperimentally, determine the slope and intercept using thefollowing equations:S 5 Ta12 Ta2#/T012 T02# (2)I 5 T013Ta2! 2 Ta13T02!#/T012 T02! (3)wher
44、e:S = slope (nominal value = 1.00),I = intercept,Ta1= reference transition temperature for Reference Mate-rial 1 taken from Table 1,Ta2= reference transition temperature for Reference Mate-rial 2 taken from Table 1,T01= experimentally observed transition onset temperaturefor Reference Material 1, an
45、dT02= experimentally observed transition onset temperaturefor Reference Material 2.(WarningThe slope S is a dimensionless number whosevalue is independent of which temperature scale is used forIand T.I, in all cases, must have the same units as Ta1, Ta2, T01,and T02that are by necessity consistent w
46、ith each other.)11.2 S should be calculated to 60.01 units while Ishould becalculated to 60.1C.11.3 Using the determined values for S and I, Eq 1 may beused to calculate the actual specimen transition, Tt, from anyexperimentally observed transition temperature, T0, for theparticular TMA instrument e
47、mployed.NOTE 11The final result is rounded to the nearest 0.1C consistentwith the repeatability standard deviation reported in 13.2.1.FIG. 2 Assignment of Extrapolated Onset Temperature (To) fromTMA Thermal Curve for Specimen Exhibiting Pretransition Soft-eningE1363 13311.4 One-Point Calibration:11.
48、4.1 In this abbreviated procedure, a relationship betweenthe extrapolated onset temperature as observed from the use ofa weighted penetration probe with one of the calibrationreference materials (see Table 1) and the temperature asassigned by a temperature sensor is established. The operatorshould c
49、hoose a calibration reference material that is near thetemperature of the transition or phenomenon under study. Forexample, if one were interested in assigning the glass transitiontemperature of a polycarbonate specimen (Tg 150C), a goodchoice for the temperature calibration reference material wouldbe indium metal (Tm = 156.6C).11.4.1.1 Using the sample handling techniques as describedin 7.1 and 10.1.2, use a penetration probe to obtain the TMAthermal curves for the calibration standard chosen in Table 1.11.4.1.2 From the known melting poi
